CN111403661A - Composite diaphragm for power lithium ion battery and preparation method thereof - Google Patents
Composite diaphragm for power lithium ion battery and preparation method thereof Download PDFInfo
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- CN111403661A CN111403661A CN202010205803.6A CN202010205803A CN111403661A CN 111403661 A CN111403661 A CN 111403661A CN 202010205803 A CN202010205803 A CN 202010205803A CN 111403661 A CN111403661 A CN 111403661A
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- lithium ion
- ion battery
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Cell Separators (AREA)
Abstract
The invention discloses a composite diaphragm for a power lithium ion battery and a preparation method thereof, belongs to the technical field of power lithium ion batteries, and is beneficial to lithium ion transmission in an aluminum oxide ceramic composite diaphragm and improvement of the multiplying power performance of the power lithium ion battery by modifying the surface of aluminum oxide through an amino modifier. The composite diaphragm is an amino-modified alumina ceramic composite diaphragm; firstly, preparing amino modified alumina powder, then preparing the amino modified alumina powder into ceramic coating slurry, then coating the slurry on the single surface or double surfaces of a polyethylene base film (5-25 mu m), obtaining a final composite diaphragm after treatment, and carrying out performance test on the obtained composite diaphragm.
Description
Technical Field
The invention belongs to the technical field of power lithium ion batteries, and particularly relates to a composite diaphragm for a power lithium ion battery and a preparation method thereof.
Background
The diaphragm is arranged inside the lithium ion battery to separate the positive electrode and the negative electrode to prevent the battery from short circuit, and a transmission channel is also required to be provided for lithium ions, so that the electrochemical performance of the lithium ion battery is influenced by the diaphragm. The polyolefin diaphragm becomes the diaphragm of the lithium ion battery which is most widely used at present because of the outstanding advantage of low production cost. However, with the development of power lithium ion batteries, higher requirements are placed on the diaphragm serving as a safety guarantee component of the lithium ion battery, and in order to increase the energy density of a single battery, the thickness of the polyolefin diaphragm is made thinner. This is a significant challenge for safe operation of the battery.
The most common method of modifying polyolefin separator membranes at present is surface coating, since this method is very simple and inexpensive and easy to process on a large scale. At present, ceramic particles (Al2O3, SiO2 and the like) and a binder (PVDF, CMC and the like) are coated on a polyolefin-based film, which is the most used in the industry, and the modification method can obviously improve the thermal stability of the diaphragm, reduce the thermal shrinkage rate of the diaphragm and improve the wettability of the diaphragm to electrolyte. However, the ionic conductivity of the composite membrane prepared by the method is generally low, and the ion migration number of the composite membrane is not obviously improved, so that the performance requirements of the lithium ion battery under the conditions of large current charging and discharging cannot be met.
Disclosure of Invention
The invention provides a composite diaphragm for a power lithium ion battery and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composite diaphragm for a power lithium ion battery is an amino-modified alumina ceramic composite diaphragm.
A preparation method of a composite diaphragm for a power lithium ion battery comprises the following steps:
(1) dispersing a certain mass of alumina powder in absolute ethyl alcohol and uniformly stirring to form a suspension;
(2) adding an alcohol-water solution of an amino modifier into the suspension obtained in the step (1), and stirring and mixing uniformly;
(3) heating the mixed solution obtained in the step (2) at 60-90 ℃ for 12-48 h;
(4) carrying out vacuum filtration, washing and drying on the mixed solution treated in the step (3) to obtain amino modified alumina powder;
(5) mixing the amino modified alumina powder obtained in the step (4) with a binder and a solvent according to a certain mass ratio, and performing ball milling for 4 hours to obtain ceramic coating slurry;
(6) coating the slurry obtained in the step (5) on the single surface or double surfaces of the base film in a blade mode;
(7) and (4) drying the ceramic composite membrane uniformly coated in the step (6) for 24 hours in vacuum at the temperature of 70-80 ℃ to obtain the amino-modified alumina ceramic composite membrane.
In the above step, the amino modifier in step (2) is one or more of KH-550, glucosamine, sulfamic acid, acrylamide, amino acid and KH-570, the volume fraction of the amino modifier in the alcohol aqueous solution of the amino modifier is 15-20%, and the mass ratio of the amino modifier to the alumina is 1: 1, the alcohol is absolute ethyl alcohol, methanol or n-butyl alcohol;
the amino modified alumina powder obtained in the step (5) is mixed with a binder, a surfactant and a solvent according to the ratio of 10-15: 1-3: 0.1-2: ball milling at a mass ratio of 80-88.9; the binder is polyvinylidene fluoride, polyacrylic acid, styrene butadiene rubber or sodium carboxymethylcellulose, the surfactant is PVP or CTAB, and the solvent is DMF, water, absolute ethyl alcohol or NMP.
In the step (6), the base film is a polyethylene base film, and the thickness of the polyethylene base film is 5-25 μm.
The composite diaphragm for the power lithium ion battery and the preparation method thereof have the beneficial effects that the composite diaphragm is an amino-modified alumina ceramic composite diaphragm, lithium ions have a solvation phenomenon in electrolyte, and polar groups and L i + have certain interaction.
Drawings
FIG. 1 shows Al in example2O3Ceramic particles and amino-modified Al2O3XPS spectra of the ceramic particles;
FIG. 2 shows PE film (a) and Al film in the examples2O3a/PE composite film (b) and N-Al2O3SEM pictures of/PE composite membranes (c, d);
FIG. 3 shows PE film (a) and Al film in the examples2O3a/PE composite film (b) and N-Al2O3Thermal stability test of the/PE composite membrane (c);
FIG. 4 illustrates L iCoO of different diaphragm assemblies in the examples2The cycling performance (a) and the rate performance (b) of the/L i button cell.
Detailed Description
The invention is described in detail below with reference to the following figures and specific examples:
example 1
A composite diaphragm for a power lithium ion battery is an amino-modified alumina ceramic composite diaphragm, wherein the amino-modified alumina ceramic is coated on the surface of a base membrane, as shown in figure 1Modified Al2O3Successfully introduces amino groups on the surface of the ceramic particles and prepares N-Al2O3The combination of the/PE composite membrane and the figure 1 and the figure 2 shows that the amino modification does not obviously change Al2O3The appearance of the ceramic particles can be uniformly distributed on the surface of the PE base film.
A preparation method of a composite diaphragm for a power lithium ion battery comprises the following steps:
(1) dispersing a certain mass of alumina powder in 50 m L absolute ethyl alcohol and uniformly stirring to form a suspension;
(2) adding an alcohol water solution with the amino acid volume fraction of 18% as an amino modifier into the suspension obtained in the step (1), stirring and mixing uniformly, wherein the mass ratio of the amino modifier to the alumina is 1: 1;
(3) transferring the mixed system obtained in the step (2) into a three-neck flask, heating to 60 ℃, and reacting for 24 hours;
(4) carrying out vacuum filtration on the mixed solution treated in the step (3) to obtain amino modified alumina powder, washing the amino modified alumina powder with ethanol and distilled water for several times respectively, and drying the amino modified alumina powder for later use;
(5) mixing the amino modified alumina powder obtained in the step (4) with a binder polyvinylidene fluoride, a surfactant PVP and a solvent DMF according to the weight ratio of 11: 2: 0.5: ball milling at the mass ratio of 86.5, and ball milling for 4 hours to obtain ceramic coating slurry;
(6) coating the slurry obtained in the step (5) on the single surface or double surfaces of a polyethylene base film (5-25 mu m) by a blade coater;
(7) and (4) putting the ceramic composite membrane uniformly coated in the step (6) into a vacuum drying oven, and drying at 70 ℃ for 24 hours to obtain a final ceramic composite membrane sample.
Example 2
The composite diaphragm is an amino-modified alumina ceramic composite diaphragm, and the amino-modified alumina ceramic is coated on the surface of a base film.
A preparation method of a composite diaphragm for a power lithium ion battery comprises the following steps:
(1) dispersing a certain mass of alumina powder in 50 m L absolute ethyl alcohol and uniformly stirring to form a suspension;
(2) adding an alcohol aqueous solution with the volume fraction of amino modifier KH-550 of 20% into the suspension obtained in the step (1), stirring and mixing uniformly, wherein the mass ratio of the amino modifier to the alumina is 1: 1;
(3) transferring the mixed system obtained in the step (2) into a three-neck flask, heating to 90 ℃, and reacting for 48 hours;
(4) carrying out vacuum filtration on the mixed solution treated in the step (3) to obtain amino modified alumina powder, washing the amino modified alumina powder with ethanol and distilled water for several times respectively, and drying the amino modified alumina powder for later use;
(5) mixing the amino modified alumina powder obtained in the step (4) with polyacrylic acid serving as a binder, CTAB serving as a surfactant and absolute ethyl alcohol serving as a solvent according to the weight ratio of 10: 1: 0.1: ball milling at the mass ratio of 80, and ball milling for 4 hours to obtain ceramic coating slurry;
(6) coating the slurry obtained in the step (5) on the single surface or double surfaces of a polyethylene base film (5-25 mu m) by a blade coater;
(7) and (4) putting the ceramic composite membrane uniformly coated in the step (6) into a vacuum drying oven, and drying at 80 ℃ for 24 hours to obtain a final ceramic composite membrane sample.
Example 3
The composite diaphragm is an amino-modified alumina ceramic composite diaphragm, and the amino-modified alumina ceramic is coated on the surface of a base film.
A preparation method of a composite diaphragm for a power lithium ion battery comprises the following steps:
(1) dispersing a certain mass of alumina powder in 50 m L absolute ethyl alcohol and uniformly stirring to form a suspension;
(2) adding an alcohol water solution with the volume fraction of amino modifier acrylamide being 15% into the suspension obtained in the step (1), stirring and mixing uniformly, wherein the mass ratio of the amino modifier to the alumina is 1: 1;
(3) transferring the mixed system obtained in the step (2) into a three-neck flask, heating to 80 ℃, and reacting for 12 hours;
(4) carrying out vacuum filtration on the mixed solution treated in the step (3) to obtain amino modified alumina powder, washing the amino modified alumina powder with ethanol and distilled water for several times respectively, and drying the amino modified alumina powder for later use;
(5) mixing the amino modified alumina powder obtained in the step (4) with a binder sodium carboxymethyl cellulose, a surfactant PVP and a solvent NMP according to a ratio of 15: 3: 2: ball milling at the mass ratio of 88.9 for 4 hours to obtain ceramic coating slurry;
(6) coating the slurry obtained in the step (5) on the single surface or double surfaces of a polyethylene base film (5-25 mu m) by a blade coater;
(7) and (4) putting the ceramic composite membrane uniformly coated in the step (6) into a vacuum drying oven, and drying at 70 ℃ for 24 hours to obtain a final ceramic composite membrane sample.
Comparative example 1
And assembling the battery by using the polyethylene base film as the diaphragm.
Comparative example 2
The ceramic composite separator was prepared in the same manner as in example 1, except that unmodified alumina was used, and the battery was assembled by using the unmodified alumina ceramic composite separator as a separator.
Treating three different membranes at 130 deg.C for 30min, as shown in FIG. 3, the amino-modified alumina ceramic composite membrane has small thermal shrinkage size, and is coated with amino-modified Al2O3After the ceramic particles, the thermal stability of the separator is improved to some extent.
Fig. 4 reflects that the cycling stability and rate capability of the button cell assembled by the amino-modified alumina ceramic composite membrane are obviously improved. The battery has the advantages that after the battery is cycled for 80 circles under the current density of 1C, the discharge capacity is not basically attenuated, and the cycling stability is best. Under the condition of 4C high-current charge and discharge, N-Al2O3The battery assembled by the PE composite membrane also keeps more than 50 percent of the initial discharge capacity, which is higher than that of the unmodified alumina ceramic composite membrane.
The foregoing is only a preferred embodiment of this invention and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the invention and these modifications should also be considered as the protection scope of the invention.
Claims (9)
1. The composite diaphragm for the power lithium ion battery is characterized by being an amino-modified alumina ceramic composite diaphragm.
2. A preparation method of a composite diaphragm for a power lithium ion battery is characterized by comprising the following steps:
(1) dispersing alumina powder in 50 m L absolute ethyl alcohol and stirring uniformly to form a suspension;
(2) adding an alcohol-water solution of an amino modifier into the suspension obtained in the step (1), and stirring and mixing uniformly;
(3) heating the mixed solution obtained in the step (2) at 60-90 ℃ for 12-48 h;
(4) carrying out vacuum filtration, washing and drying on the mixed solution treated in the step (3) to obtain amino modified alumina powder;
(5) mixing the amino modified alumina powder obtained in the step (4) with a binder, a surfactant and a solvent according to a certain mass ratio, and performing ball milling for 4 hours to obtain ceramic coating slurry;
(6) coating the slurry obtained in the step (5) on the single surface or double surfaces of the base film in a blade mode;
(7) and (4) drying the ceramic composite membrane uniformly coated in the step (6) for 24 hours in vacuum at the temperature of 70-80 ℃ to obtain the amino-modified alumina ceramic composite membrane.
3. The preparation method of the composite separator for the power lithium ion battery according to claim 2, wherein the volume fraction of the amino modifier in the alcohol aqueous solution of the amino modifier in the step (2) is 15% to 20%.
4. The preparation method of the composite separator for the power lithium ion battery according to claim 2, wherein the mass ratio of the amino modifier in the step (2) to the alumina in the step (1) is 1: 1.
5. the preparation method of the composite separator for the power lithium ion battery according to claim 2 or 3, wherein the amino modifier in the step (2) is one or more of KH-550, glucosamine, sulfamic acid, acrylamide, amino acid and KH-570, and the alcohol is absolute ethyl alcohol, methanol or n-butanol.
6. The preparation method of the composite separator for the power lithium ion battery according to claim 2, wherein the amino-modified alumina powder in the step (5) is mixed with a binder, a surfactant and a solvent according to a ratio of 10-15: 1-3: 0.1-2: 80 to 88.9 mass ratio.
7. The method for preparing the composite separator for the power lithium ion battery according to claim 2 or 6, wherein the binder is polyvinylidene fluoride, polyacrylic acid, styrene butadiene rubber or sodium carboxymethylcellulose, the surfactant is PVP or CTAB, and the solvent is DMF, water, absolute ethyl alcohol or NMP.
8. The method for preparing the composite separator for the power lithium ion battery according to claim 2, wherein the base film in the step (6) is a polyethylene base film.
9. The method for preparing the composite separator for a power lithium ion battery according to claim 8, wherein the thickness of the polyethylene-based film is 5 to 25 μm.
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| CN202010205803.6A CN111403661A (en) | 2020-03-23 | 2020-03-23 | Composite diaphragm for power lithium ion battery and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112133867A (en) * | 2020-08-17 | 2020-12-25 | 浙江工业大学 | Self-assembled monolayer modified alumina diaphragm and preparation and application thereof |
| CN114824647A (en) * | 2022-05-20 | 2022-07-29 | 江苏厚生新能源科技有限公司 | Lithium ion battery diaphragm based on aluminum hydroxide coaxial nanotube and preparation method thereof |
| CN115000627A (en) * | 2022-06-17 | 2022-09-02 | 岳阳耀宁新能源科技有限公司 | Lithium ion battery diaphragm coating and application thereof |
| CN115149069A (en) * | 2022-06-20 | 2022-10-04 | 岳阳耀宁新能源科技有限公司 | Assembling method of laminated lithium battery and laminated lithium battery |
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Cited By (6)
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|---|---|---|---|---|
| CN112133867A (en) * | 2020-08-17 | 2020-12-25 | 浙江工业大学 | Self-assembled monolayer modified alumina diaphragm and preparation and application thereof |
| CN112133867B (en) * | 2020-08-17 | 2023-04-07 | 浙江工业大学 | Self-assembled monolayer modified alumina diaphragm and preparation and application thereof |
| CN114824647A (en) * | 2022-05-20 | 2022-07-29 | 江苏厚生新能源科技有限公司 | Lithium ion battery diaphragm based on aluminum hydroxide coaxial nanotube and preparation method thereof |
| CN114824647B (en) * | 2022-05-20 | 2023-09-29 | 江苏厚生新能源科技有限公司 | Lithium ion battery diaphragm based on aluminum hydroxide coaxial nanotubes and preparation method thereof |
| CN115000627A (en) * | 2022-06-17 | 2022-09-02 | 岳阳耀宁新能源科技有限公司 | Lithium ion battery diaphragm coating and application thereof |
| CN115149069A (en) * | 2022-06-20 | 2022-10-04 | 岳阳耀宁新能源科技有限公司 | Assembling method of laminated lithium battery and laminated lithium battery |
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Application publication date: 20200710 |